18 results about "P-chloronitrobenzene" patented technology

The invention belongs to the technical field of preparation of nano noble metal catalysts, and relates to a preparation method of a doped carbon-based nano noble metal catalyst. Phytic acid doped polyaniline is prepared through chemical oxidative polymerization, a nitrogen and phosphorus co-doped carbon carrier is obtained through pyrolysis under the nitrogen atmosphere, gold and palladium bimetal is loaded through a metal colloid adsorption method, the doped carbon-based nano noble metal catalyst is obtained, the introduced doped element phosphorus has anchoring and dispersing effects on noble metal, and the noble metal is more stable in performance. The activity of the catalyst is remarkably improved by introducing a trace amount of second component metal palladium. The catalyst prepared by the invention is simple in synthesis method, high in activity, good in selectivity and excellent in cycling stability, is suitable for preparing parachloroaniline by hydrogenation of parachloronitrobenzene, and has a relatively wide application prospect.

The present application relates to the technical field of chemical synthesis, in particular to a method for inhibiting poisoning of a proton exchange membrane in one-pot production of p-chlorophenylhydrazine, which uses p-chloronitrobenzene as a substrate and tin dichloride for reduction reaction to realize one-pot synthesis process of p-chlorophenylhydrazine.The method does not need intermediate separation steps, can directly feed materials, effectively reduces loss of raw materials, and realizes continuous reduction of tin tetrachloride by reasonable inhibition of poisoning of the proton exchange membrane, recycles tin dichloride, and re-puts it into the nitrobenzene reduction step.Compared with the traditional method, the method solves the yield reduction problem caused by p-chlorophenylhydrazine preparation in steps and purification, solves the problem of poisoning of the proton exchange membrane by phenylhydrazine hydrochloride, is suitable for industrial production environment, improves the product yield, reduces environmental pollution, has low cost, and is suitable for efficient continuous production of important chemical intermediate p-chlorophenylhydrazine.

The application discloses a kind of rich vacancy molybdenum disulfide catalyst and preparation method and purposes, and preparation method is as follows:1) according to the proportion of 1-5mg / mL, molybdenum disulfide powder is mixed with deionized water, and molybdenum disulfide water dispersion is obtained;2) molybdenum disulfide water dispersion obtained in step 1) is loaded into the hydrothermal kettle with polytetrafluoroethylene lining, and sealed;Hydrothermal reaction is carried out at 140-190 DEG C for 4-20h;Drop to room temperature, centrifugal, dry, and obtain rich vacancy molybdenum disulfide catalyst.The method of the application is simple, efficient, green and pollution-free, and easy to scale up.The rich vacancy molybdenum disulfide catalyst prepared by the application has rich active sites, and the catalytic activity in the field of substituted nitrobenzene hydrogenation can be significantly improved due to the increase of active site sulfur vacancy, which is used for the hydrogenation catalysis of p-chloronitrobenzene, and the conversion rate of p-chloronitrobenzene is 100%, and the selectivity of p-chloroaniline is 100%.The performance of the catalyst exceeds that of raw material molybdenum disulfide.

The present invention provides a method for recovering and treating a 4,4-dinitrodiphenyl ether by-product, and belongs to the technical field of organic synthesis. The present invention adjusts the pH value to 3-4 to remove substances that can react with acid in the by-product salt, and the functions of ferrous sulfate and the first activated carbon are to decolorize and remove the color of the 4,4-dinitrodiphenyl ether material. The pH value is then adjusted to 6-8 to remove ferrous sulfate, and then a second decolorization is performed to obtain a white solid salt. The function of hydrogen peroxide is to remove organic matter in the reaction, and the resin column elution ensures that p-chloronitrobenzene, sodium p-nitrophenolate, and DNP organic matter are completely removed. Finally, a solid salt having a sodium chloride content of ≥99.1g / 100g and a TOC (total organic carbon) of less than 50mg / kg is obtained. The obtained solid salt does not have the odor of p-nitrochlorobenzene, meets the industrial salt standard, and realizes the recovery and use of the 4,4-dinitrodiphenyl ether by-product, thereby reducing costs.

The invention belongs to the field of water treatment, and relates to a method for intensively removing parachloronitrobenzene in water after removing phosphorus pollution in water by using nano zero-valent iron. The method comprises the following steps: adding nano zero-valent iron into phosphorus-containing to-be-treated water, carrying out a stirring reaction to remove phosphorus in the water, then adding parachloronitrobenzene-containing to-be-treated water, and continuously carrying out a stirring reaction to remove parachloronitrobenzene in the water. The invention provides a novel and efficient method for removing parachloronitrobenzene in water, nanoscale zero-valent iron is used for removing phosphorus and organic pollutants, parachloronitrobenzene can be rapidly and efficiently removed, and the method can adapt to a wide pH value range. The phosphorylated nano zero-valent iron generated in situ after phosphorus removal of the nano zero-valent iron has good reduction performance, and parachloronitrobenzene in water can be efficiently removed. Meanwhile, the nZVI in the method can remove phosphorus and parachloronitrobenzene pollution in water at the same time, the effect of treating waste with waste can be achieved, operation is easy, and the method has wide application prospects.

The invention relates to the technical field of chemical synthesis, and particularly discloses a catalyst, a preparation method thereof and a process method for producing 3, 4-dichloronitrobenzene without wastewater, and the process method for producing 3, 4-dichloronitrobenzene without wastewater comprises the following steps: (1) adding a self-dehydration solid acid catalyst into a first-stage chlorination tower, a second-stage chlorination tower and a third-stage chlorination tower; (2) a parachloronitrobenzene raw material is sequentially conveyed into a first-stage chlorination tower, a second-stage chlorination tower and a third-stage chlorination tower, chlorine is introduced for a chlorination reaction, generated hydrogen chloride gas and unreacted chlorine escape from the tower tops and enter a tail gas main pipeline, and reacted chlorination liquid is sequentially conveyed into a first-stage deacidification kettle and a second-stage deacidification kettle for deacidification treatment; (3) hydrogen chloride gas and unreacted chlorine gas in the tail gas main pipeline are discharged after being treated to reach the standard; and (4) treating the deacidified chlorination liquid through a light component removal tower and a heavy component removal tower in sequence, crystallizing and purifying to obtain 3, 4-dichloronitrobenzene.

The invention relates to the technical field of 4, 4 '-diaminodiphenylamine, in particular to a synthesis process of 4, 4'-diaminodiphenylamine, which comprises the following steps: dissolving parachloronitrobenzene, paranitroaniline and alkali in an organic solvent, heating, stirring, pouring into ice water, filtering, washing and drying to obtain 4, 4 '-dinitrodiphenylamine; adding the mixture, a catalyst and an organic solvent into a high-pressure reaction kettle, introducing hydrogen after nitrogen replacement, heating and stirring, filtering the catalyst after the reaction is finished, and recovering and reusing the catalyst; according to the synthesis process of 4, 4 '-diaminodiphenylamine adopting the steps, the reaction process is shortened, the steps of separation and purification of intermediate products are reduced, the production efficiency is improved, the loss in the production process is reduced, and the product with high purity and high yield is obtained.

The application discloses N-o-tolyl-N'-(1-methyl-2-benzyl) ethyl p-phenylenediamine and a preparation method and application thereof. The product is prepared from p-chloronitrobenzene and 2-methylaniline through a nucleophilic substitution reaction to obtain N-o-tolyl p-nitroaniline, and then the N-o-tolyl p-nitroaniline and benzylacetone are subjected to a catalytic reduction reaction under high temperature and high pressure conditions to obtain the final product. The product has excellent ozone protection effect and anti-crack performance, and can obviously improve the red discoloration phenomenon of the tire side caused by the migration of the antioxidant.

The application belongs to the field of medicine, and discloses a compound with the structure of formula I, a preparation method of the compound, and the compound is a pyrazole acylhydrazine derivative containing a diphenyl ether unit, which is obtained by substituting p-chloronitrobenzene with phenol, and then by reduction, diazotization, re-reduction, hydrochloric acid removal and hydrazide reaction; the pyrazole acylhydrazine derivative containing the diphenyl ether unit has obvious inhibitory effect on human pancreatic cancer cells, human breast cancer cells and human gastric cancer cells, and can be used as a potential new type of antitumor candidate drug molecule.

The present invention provides a Pt / NiZnFe-LDH@C3N4 catalyst, a preparation method thereof and an application thereof. The catalyst comprises a carrier and active metal nanoparticles supported on the carrier, and the carrier is an organic-inorganic composite carrier composed of g-C3N4 and NiZnFe-LDH. Preferably, the active metal is Pt. This catalyst is applied to the reaction of catalytic hydrogenation of p-chloronitrobenzene to produce p-chloroaniline, and both the conversion rate of p-chloronitrobenzene and the selectivity of p-chloroaniline can reach 99.99%. Pt / NiZnFe-LDH@C3N4 is used to catalyze the hydrogenation of different chloronitrobenzenes to prepare the corresponding aniline compounds, and the selectivity of the target products is all above 99.9%. This novel Pt / NiZnFe-LDH@C3N4 catalyst has a novel catalyst structure, is green and environmentally friendly, and has excellent industrial practical value.

The present invention belongs to the technical field of the preparation of nano noble metal catalysts, and relates to a preparation method of a doped carbon-based nano noble metal catalyst. In the present invention, phytic acid-doped polyaniline is prepared by chemical oxidative polymerization, and a nitrogen and phosphorus co-doped carbon carrier is obtained by pyrolysis under a nitrogen atmosphere. Gold and palladium bimetals are loaded by a metal colloid adsorption method to obtain a doped carbon-based nano noble metal catalyst. The introduced doped element phosphorus has an anchoring and dispersing effect on the noble metal, and the introduced trace second component metal palladium significantly improves the activity of the catalyst. The catalyst prepared by the present invention has a simple synthesis method, high activity, good selectivity, excellent cyclic stability, is applicable to the hydrogenation of p-chloronitrobenzene to prepare p-chloroaniline, and has a broad application prospect.

The present invention discloses a preparation method of 4,4'-dinitrodiphenyl ether. By using a one-pot method and a polar organic solvent as the reaction solvent, the raw material p-chloronitrobenzene and the catalyst are first pre-reacted to form an ester, then a carbonate auxiliary agent is added, and etherification occurs under an inert atmosphere to prepare 4,4'-dinitrodiphenyl ether. After filtration, the filtrate is decolorized, subjected to vacuum distillation, and alcohol precipitation to obtain the target product, and the mother liquor solvent is recovered and the kettle residue is recycled. The reaction of the present invention is simple and easy to control, has a short reaction time, few side reactions, and realizes the centralized treatment of organic waste, reducing the difficulty of post-treatment. All solvents involved in the whole process are recycled, the produced target product has a low cost and high purity, and the total yield reaches over 96.5%.

The invention relates to a method for green and efficient preparation of 3-amino-4 '-nitrodiphenyl ether, and belongs to the technical field of organic synthesis. The method for preparing 3-amino-4 '-nitrodiphenyl ether comprises the following steps: S1, reacting a hydrogen bond acceptor and a hydrogen bond donor under a heating condition to prepare DES; and S2, adding parachloronitrobenzene and m-aminophenol into the DES prepared in the step S1, heating to carry out etherification reaction, and carrying out water washing and solid-liquid separation treatment on the reaction liquid to obtain the 3-amino-4 '-nitrodiphenyl ether product. The hydrogen bond receptor is at least one of choline chloride and betaine; the hydrogen bond donor is at least one of polyethylene glycol, urea and thiourea. The method for preparing the 3-amino-4 '-nitrodiphenyl ether has the advantages of mild reaction conditions, environmental friendliness and the like, and the 3-amino-4'-nitrodiphenyl ether product with high yield and high purity can be directly obtained.

The application discloses a preparation method and application of a nitrogen and phosphorus doped carbon coated metal structure catalyst, and comprises the following steps: according to the mass ratio of microorganisms, biomass and water, 0.1-10 g:10-50 g:10-50 g of corresponding substances are weighed and mixed and stirred, and a metal impregnation solution (for example, [PdCl4] 2‑ , [NiCl4] 2‑ , [CoCl4] 2‑ , [RuCl4] 2‑ , etc.) is added, and then a nitrogen and phosphorus doped carbon coated metal palladium catalyst (the total loading amount of N and P of the catalyst is 1.0-6.0%, and the loading amount of the metal is 0.5-8%) is obtained through hydrothermal carbonization, pyrolysis or microwave, etc. The application adopts the biomass and microorganism interaction to further form a nitrogen and phosphorus doped carbon coating layer, and the nitrogen and phosphorus doped carbon coating layer has a stronger interaction with palladium or other metals, and shows the characteristics of high activity, selectivity and acid resistance in a chloronitrobenzene hydrogenation reaction.

The invention relates to the technical field of chemical synthesis, and particularly discloses a catalyst, a preparation method of the catalyst and a continuous chlorination production process of 3, 4-dichloronitrobenzene. The continuous chlorination production process of 2, 4-dichloronitrobenzene comprises the following steps: (1) adding a hierarchical porous supported metal chloride catalyst into a first-stage chlorination tower, a second-stage chlorination tower and a third-stage chlorination tower; (2) a parachloronitrobenzene raw material is sequentially conveyed into a first-stage chlorination tower, a second-stage chlorination tower and a third-stage chlorination tower, chlorine is introduced for a chlorination reaction, generated hydrogen chloride gas and unreacted chlorine escape from the tower tops and enter a tail gas main pipeline, and reacted chlorination liquid is sequentially conveyed into a first-stage deacidification kettle and a second-stage deacidification kettle for deacidification treatment; and (3) conveying the deacidified chlorination liquid into a light component removal tower to distill out parachloronitrobenzene for recycling, treating a tower kettle material in a heavy component removal tower, extracting tar from the tower kettle, and crystallizing and purifying a tower top material to obtain 3, 4-dichloronitrobenzene.

This invention relates to a method for synthesizing hydroquinone, a pharmaceutical and chemical intermediate. The invention comprises the following steps: (1) hydrolysis of p-chloronitrobenzene in an alkaline solution, adjusting the pH to 5-6 with acid to obtain p-nitrophenol; (2) reduction of p-nitrophenol and hydrogen under catalytic conditions to obtain p-aminophenol; (3) diazotization of a dilute acid solution of p-aminophenol with sodium nitrite; the reaction solution reacts with a dilute acid solution used for hydrolysis to obtain hydroquinone; after the reaction, solvent extraction is performed, followed by concentration, centrifugation, and drying. The reactions are carried out in a microreactor system. Compared with existing hydroquinone production processes, this invention uses continuous flow technology for continuous production, greatly improving production efficiency and saving production costs. It solves the problems of high levels of waste, low selectivity, and high purification costs associated with traditional batch processes. Furthermore, the continuous flow production process has a lower scale-up effect, easier process control, and is suitable for industrial production.

The present application relates to the technical fields of chemical synthesis, and discloses a kind of catalyst and preparation method and the continuous chlorination production process of 3,4-dichloronitrobenzene, wherein the continuous chlorination production process of 3,4-dichloronitrobenzene includes the following steps: (1) adding multi-stage channel supported metal chloride catalyst into primary chlorination tower, secondary chlorination tower and tertiary chlorination tower; (2) feeding p-chloronitrobenzene raw material into primary chlorination tower, secondary chlorination tower and tertiary chlorination tower in sequence and introducing chlorine gas for chlorination reaction, the generated hydrogen chloride gas and unreacted chlorine gas escape from the top of the tower, enter the tail gas main pipeline, and the reacted chlorination liquid is fed into primary deacidification kettle and secondary deacidification kettle in sequence for deacidification treatment; (3) the deacidified chlorination liquid is fed into light-removing tower to distill p-chloronitrobenzene for recycling, the tower kettle material is fed into heavy-removing tower for treatment, tar is recovered from the tower kettle, and 3,4-dichloronitrobenzene is obtained by crystallization and purification of the tower top material.

The present application relates to the technical fields of chemical synthesis, and discloses a kind of catalyst and preparation method and the process method of wastewater-free production 3,4-dichloronitrobenzene, wherein the process method of wastewater-free production 3,4-dichloronitrobenzene includes the following steps: (1) adding self-dehydration type solid acid catalyst to primary chlorination tower, secondary chlorination tower, tertiary chlorination tower;(2) the p-chloronitrobenzene raw material is sequentially transported to primary chlorination tower, secondary chlorination tower, tertiary chlorination tower and is introduced into chlorine gas to carry out chlorination reaction, the generated hydrogen chloride gas and unreacted chlorine gas escape from tower top, enter exhaust gas main pipeline, and the chlorinated liquid of reaction is sequentially transported to primary deacidification kettle and secondary deacidification kettle to carry out deacidification treatment;(3) hydrogen chloride gas and unreacted chlorine gas in exhaust gas main pipeline are discharged after treatment reaches standard;(4) deacidification chlorinated liquid is sequentially treated by light removal tower and heavy removal tower, crystallization purification, and 3,4-dichloronitrobenzene is obtained.